CN114920578A - Preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage - Google Patents

Preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage Download PDF

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CN114920578A
CN114920578A CN202210849814.7A CN202210849814A CN114920578A CN 114920578 A CN114920578 A CN 114920578A CN 202210849814 A CN202210849814 A CN 202210849814A CN 114920578 A CN114920578 A CN 114920578A
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parts
anorthite
gehlenite
porous
ceramic
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CN114920578B (en
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袁飞
杨琳梓
张辉
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Zibo Jinshiwang Technology Ceramic Group Co ltd
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Zibo Jinshiwang Technology Ceramic Group Co ltd
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Abstract

The invention belongs to the technical field of ceramic preparation, and particularly relates to a preparation method of porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate. Weighing ingredients according to a certain mass part ratio, wherein the ingredients comprise feldspar, quartz, waste glass powder, waste brick powder, kaolin, sawdust, sodium tripolyphosphate, polyacrylic acid, calcium carbonate, alumina, fused mullite powder, silicon carbide and talc, adding water into the ingredients for ball milling, drying slurry, manufacturing material particles, sieving with a 100-mesh sieve, and taking the material particles which are sieved with the 100-mesh sieve; molding the material particles by compression, and drying to obtain a blank body; and heating the blank to 1170 ℃, firing, and cooling to room temperature to prepare the anorthite/gehlenite complex-phase ceramic. The preparation method of the anorthite/gehlenite complex phase ceramic provided by the invention has the advantages that the selected raw materials are mostly mineral materials, the cost is low, the process is simple, and the industrial production is easy to realize.

Description

Preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage
Technical Field
The invention belongs to the technical field of ceramic preparation, and particularly relates to a preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage rate.
Background
Anorthite has a high melting point, low thermal conductivity and thermal expansion coefficient and excellent thermal shock resistance. The porous ceramic taking anorthite as a main crystal phase has wide application prospects in the aspects of sewage treatment, sound absorption, high-temperature gas-solid separation, high-temperature heat insulation, gas sensors, catalyst carriers and the like. CN201510649256.X and CN201811276561.9 report that the porous anorthite ceramic prepared by a foam gel injection method has high porosity, but the process conditions are harsh and difficult to control; CN201810985266.4 reports a method for preparing porous ceramics by adding a pore-forming agent, the size and the shape of pores are controllable, the process is simple, but the pore distribution uniformity of the prepared anorthite sample is poor. The anorthite ceramic has low strength and is difficult to meet the requirements of some severe conditions; meanwhile, machining cracks are brought to products by mechanical processing after firing of ceramic products, so that control of firing precision is very important, and research on low firing shrinkage rate, particularly research on improvement of pore structure, density, volume shrinkage rate and mechanical property of porous ceramics through optimization of formula and process conditions, becomes increasingly important. The gehlenite has small density, small thermal expansion coefficient, low thermal conductivity and high strength and water resistance, for example, CN202010669868.6 mentions that the gehlenite can be compounded with the gehlenite to generate complex phase ceramic, so that the physical, mechanical and harsh environment-resistant service performance of the gehlenite can be enhanced.
The physical and chemical reactions of the materials in the sintering process of the solid ceramic blank change the microstructure and the phase, the viscosity of the glass phase is reduced in the high-temperature sintering process, the space between the solid materials is shortened, the contact area is increased, the bonding strength is increased, and the macroscopic expression is shrinkage, densification and strength increase. Therefore, the material formula and the sintering process have obvious influence on the microstructure and the macroscopic performance index of the ceramic material. In the production process of the porous ceramic, the reduction of the shrinkage rate and the improvement of the porosity rate are usually at the expense of the mechanical performance index, and the shrinkage rate, the porosity rate and the mechanical performance are difficult to be effectively unified. In the glass phase, the generation of the anorthite and the anorthite needs the processes of substance diffusion, crystal generation and growth, and pores generated in the low-temperature decomposition process of the pore-forming agent form obstacles to the substance diffusion and crystallization processes. The problems need to continuously design and optimize the formula composition and the sintering process, and deeply research the evolution, generation and mutual law of phases. Only by optimizing the formula composition and balancing the competition process among the generation of the pores, anorthite and gehlenite can the microstructure be optimized to improve the firing shrinkage, so that the firing precision and the mechanical property of the ceramic product are improved simultaneously. However, no research on the firing of porous anorthite/gehlenite complex-phase ceramics with low firing shrinkage has been reported so far.
Disclosure of Invention
The purpose of the invention is: provides a preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage. The preparation method ensures the strength of the porous anorthite/gehlenite complex-phase ceramic under the condition of meeting the requirements of a pore structure, a sintering shrinkage rate and density, so as to adapt to the mechanical requirements on the porous ceramic material in different application fields.
The preparation method of the porous anorthite/gehlenite complex phase ceramic with low sintering shrinkage comprises the following steps:
(1) weighing ingredients according to a certain mass part ratio, wherein the ingredients comprise feldspar, quartz, waste glass powder, waste brick powder, kaolin, sawdust, sodium tripolyphosphate, polyacrylic acid, calcium carbonate, alumina, fused mullite powder, silicon carbide and talc; adding water into the ingredients for ball milling, then drying the obtained slurry, finally manufacturing material particles, sieving the material particles by a 100-mesh sieve, and taking the material particles which are sieved by the 100-mesh sieve;
(2) putting the material particles prepared in the step (1) into a die for compression molding, and drying to prepare a blank;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃, sintering, and cooling to room temperature to prepare the porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage.
Wherein:
the ingredients in the step (1) comprise the following raw materials in parts by weight: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of saw dust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 9.96-18.11 parts of fused mullite powder, 0.33-0.66 part of silicon carbide and 3.32 parts of talc.
In the step (1), a raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid has the main chemical composition of 3.98% of CaO and Al 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO measured as sulphate 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62%。
The mass part ratio of the ingredients to the water in the step (1) is 100: 80.
And (2) adding water into the ingredients in the step (1) and carrying out ball milling for 1h at the speed of 400 r/min.
And (2) drying the obtained slurry in the step (1) at 110 ℃ for 2 h.
The mode for manufacturing the material particles in the step (1) is manual granulation or mechanical granulation.
In the step (2), the forming pressure is 200MPa, the drying temperature is 110 ℃, and the drying time is 2 h.
In the step (3), the temperature is increased to 1170 ℃ at the speed of 6 ℃/min for sintering, and the temperature is kept for 2 h.
The cooling to room temperature in the step (3) is furnace cooling.
Wherein, the feldspar, the quartz and the waste glass powder in the ingredients provide guarantee for the generation of a glass phase in the high-temperature sintering process of the porous anorthite/gehlenite complex-phase ceramic. Calcium oxide generated by decomposing calcium carbonate reacts with alumina and silicon dioxide in materials in the firing process to generate anorthite/anorthite crystalline phase, the nucleation, growth and densification processes of the crystalline phase in the anorthite/anorthite complex-phase ceramic can be regulated and controlled in a high-temperature liquid phase by changing the using amounts of the electric-melting mullite powder and the silicon carbide, and the firing shrinkage, the pore structure, the density and the mechanical strength performance of the porous anorthite/anorthite complex-phase ceramic are optimized.
As a preferred technical scheme, the preparation method of the porous anorthite/gehlenite complex phase ceramic with low sintering shrinkage rate comprises the following steps:
(1) the materials are prepared according to the following mass portion: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of saw dust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 9.96-18.11 parts of fused mullite powder, 0.33-0.66 part of silicon carbide and 3.32 parts of talc, wherein the main chemical composition of a raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of saw dust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid is 3.98% of CaO and Al 2 O 3 12.1%、 SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO measured as sulphate 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62 percent of water is added, the mass part ratio of the ingredients to the water is 100:80, the slurry is dried for 2 hours at the temperature of 110 ℃ after ball milling is carried out for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, material particles are manufactured, and the material particles which are sieved by a 100-mesh sieve are taken out;
(2) putting the material particles prepared in the step (1) into a mold, forming under 200MPa, and drying at 110 ℃ for 2 hours to prepare a blank;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃ at the speed of 6 ℃ per minute, preserving the heat for 2 hours, and cooling to room temperature to obtain the porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the porous anorthite/gehlenite complex phase ceramic with low sintering shrinkage rate, disclosed by the invention, has the advantages that the selected raw materials are mostly mineral materials, the cost is low, the technological process is consistent with the traditional ceramic production process, the process is simple, and the industrial production is easy to realize. The porous anorthite/gehlenite complex-phase ceramic produced by the method has low firing shrinkage, can be regulated and controlled by changing the formula composition, and meets the requirements of different application fields on firing shrinkage and firing precision; the porous anorthite/gehlenite complex-phase ceramic prepared by the method has high glass phase content, the glass phase is used as a bonding phase after the anorthite/gehlenite is generated in the high-temperature sintering process, crystals in a blank body are connected with each other, and the strength of the porous anorthite/gehlenite complex-phase ceramic is ensured under the conditions of meeting the pore structure, the sintering shrinkage rate and the density, so that the porous anorthite/gehlenite complex-phase ceramic meets the mechanical requirements on porous ceramic materials in different application fields.
(2) The firing shrinkage rate of the porous anorthite/gehlenite complex-phase ceramic produced by the method can be regulated according to a process formula, the firing precision requirement of the ceramic product can be met due to low firing shrinkage rate, and the basic requirements of application fields such as solid/gas separation, solid/liquid separation, sound insulation, heat preservation and insulation, catalyst carriers and the like can be met due to high mechanical strength.
Drawings
FIG. 1 is an XRD spectrum of the porous anorthite/gehlenite complex-phase ceramic prepared in example 1;
FIG. 2 is a SEM photograph of the porous anorthite/gehlenite composite ceramic prepared in example 1;
FIG. 3 is an XRD spectrum of the porous anorthite/gehlenite complex phase ceramic prepared in example 2;
FIG. 4 is a SEM photograph of the porous anorthite/gehlenite composite ceramic prepared in example 2;
FIG. 5 is an XRD spectrum of the porous anorthite/gehlenite complex-phase ceramic prepared in example 3;
FIG. 6 is a SEM photograph of the porous anorthite/gehlenite composite ceramic prepared in example 3;
FIG. 7 is an XRD spectrum of the porous anorthite/gehlenite complex-phase ceramic prepared in comparative example 1;
FIG. 8 is a SEM photograph of the porous anorthite/gehlenite composite ceramic prepared in comparative example 1;
FIG. 9 is an XRD spectrum of the porous anorthite/gehlenite complex-phase ceramic prepared in the comparative example 2;
fig. 10 is a scanning electron microscope SEM photograph of the porous anorthite/gehlenite complex phase ceramic prepared in comparative example 2.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The preparation method of the porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate described in the embodiment 1 comprises the following steps:
(1) the materials are prepared according to the following mass portion ratio: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of saw dust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 9.96 parts of fused mullite powder, 0.66 part of silicon carbide and 3.32 parts of talc, and adding water, wherein the mass part ratio of the ingredients to the water is 100:80, the slurry is dried for 2 hours at 110 ℃ after being ball-milled for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, material particles are manually manufactured, and the material particles below a 100-mesh sieve are taken;
(2) putting the material particles prepared in the step (1) into a mold, forming under 200MPa, and drying at 110 ℃ for 2 hours to prepare a blank;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃ at the speed of 6 ℃ per minute, preserving the heat for 2 hours, and cooling to room temperature to prepare the porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate.
Wherein:
in the step (1), 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, silicon carbide and silicon carbide are mixed,The main chemical composition of the raw material mixture consisting of 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid is 3.98 percent of CaO and Al 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO in sulfate form 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62%。
The waste brick powder is analyzed by X-ray diffraction, and the phases of the ceramic are anorthite (JCPDS number 41-1486) and gehlenite (JCPDS number 01-0982), as shown in the attached figure 1. The microstructure of the ceramic is seen in scanning electron microscope SEM pictures, as shown in figure 2, the grain size is uniform, the sintering compactness is good, and a part of sintering necks have a small amount of air holes. The porous anorthite/gehlenite complex-phase ceramic has the density of 1.37 g/cubic centimeter and the open porosity of 49.69 percent according to the test by the boiling method mentioned in the national standard GB/T3810.1-2006 ceramic tile test method. The flexural strength of the ceramic measured by the three-point bending method was 19.36 MPa. The volume of the blank prepared by the step (2) is V 0 When the volume of the ceramic obtained in step (3) is V, the volume shrinkage ratio ((V) 0 -V)×100%/V 0 ) Comprises the following steps: 8.07 percent.
Example 2
The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate described in this embodiment 2 includes the following steps:
(1) the materials are prepared according to the following mass portion ratio: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 18.11 parts of fused mullite powder, 0.66 part of silicon carbide and 3.32 parts of talc, and water are added to ensure that the mass part ratio of the ingredients to the water is 100:80, and after ball milling is carried out in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour, the slurry is dried for 2 hours at the temperature of 110 degrees, material particles are manually manufactured, and the material particles below a 100-mesh sieve are taken;
(2) putting the material particles prepared in the step (1) into a mold, forming under 200MPa, and drying at 110 ℃ for 2 hours to prepare a blank;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃ at the speed of 6 ℃ per minute, preserving the heat for 2 hours, and cooling to room temperature to prepare the porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate.
Wherein:
in the step (1), a raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid has the main chemical composition of 3.98% of CaO and Al 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO measured as sulphate 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62%。
The waste brick powder is analyzed by X-ray diffraction, and the phases of the ceramics are anorthite (JCPDS number 41-1486) and gehlenite (JCPDS number 01-0982), as shown in the attached figure 3. The microstructure of the ceramic is shown in scanning electron microscope SEM picture, as shown in figure 4, the grain size is uniform, the sintering degree is moderate, and the sintering neck compactness is high. According to the test of the boiling method mentioned in the national standard GB/T3810.1-2006 ceramic tile test method, the density of the porous anorthite/gehlenite complex phase ceramic is 1.35 g per cubic centimeter, and the open porosity is 50.25%. The flexural strength of the ceramic measured by the three-point bending method was 18.26 MPa. The volume of the green body prepared by the step (2) is V 0 When the volume of the ceramic obtained in step (3) is V, the volume shrinkage ratio ((V) 0 -V)×100%/V 0 ) Comprises the following steps: 4.56 percent.
Example 3
The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate described in this embodiment 3 includes the following steps:
(1) the materials are prepared according to the following mass portion ratio: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 9.96 parts of fused mullite powder, 0.33 part of silicon carbide and 3.32 parts of talcum, and water is added to ensure that the mass part ratio of the materials to the water is 100:80, the slurry is dried for 2 hours at 110 ℃ after being ball-milled for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, material particles are manually manufactured, and the material particles below a 100-mesh sieve are taken;
(2) putting the material particles prepared in the step (1) into a mold, forming under 200MPa, and drying at 110 ℃ for 2 hours to prepare a blank;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃ at the speed of 6 ℃ per minute, preserving the heat for 2 hours, and cooling to room temperature to obtain the porous anorthite/gehlenite complex-phase ceramic.
Wherein:
in the step (1), a raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid comprises 3.98% of CaO and 0.32% of Al in main chemical composition 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO in sulfate form 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62%。
The phases of the ceramics are anorthite (JCPDS number 41-1486) and gehlenite (JCPDS number 01-0982) as shown in FIG. 5. The microstructure of the ceramic is seen in scanning electron microscope SEM pictures, as shown in figure 6, the holes are uniform and continuous, the grain size is small, and the sintering neck is compact and smooth. The test is carried out according to the steps of the boiling method mentioned in the national standard GB/T3810.1-2006 ceramic brick test method, and the porous anorthite/gehlenite complex phase is testedThe density of the ceramic was 1.32 grams per cubic centimeter and the open porosity was 51.02%. The flexural strength of the ceramic measured by the three-point bending method was 19.73 MPa. The volume of the blank prepared by the step (2) is V 0 When the volume of the ceramic obtained in step (3) is V, the volume shrinkage ratio is ((V) 0 -V)×100%/V 0 ) Comprises the following steps: 4.31 percent.
Comparative example 1
The preparation method of the porous anorthite/gehlenite complex phase ceramic in the comparative example 1 is different from the preparation method in the example 1 in that only the mass part of the electric melting mullite powder is changed into 0, namely the electric melting mullite powder is not added, and the preparation method specifically comprises the following steps:
(1) the materials are prepared according to the following mass portion ratio: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 0.66 part of silicon carbide and 3.32 parts of talcum are added, the mass part ratio of the ingredients to the water is 100:80, the slurry is dried for 2 hours at 110 ℃ after being ball-milled for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, material particles are manually manufactured, and the material particles below a 100-mesh sieve are taken;
(2) placing the material particles prepared in the step (1) into a mold, forming under 200MPa, and drying at 110 ℃ for 2 hours to prepare a blank body;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃ at the speed of 6 ℃ per minute, preserving the heat for 2 hours, and cooling to room temperature to obtain the porous anorthite/gehlenite complex-phase ceramic.
Wherein:
the raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid in the step (1) mainly comprises 3.98% of CaO and Al 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% by weight of sulfuric acidSO of salt metering 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62 percent. The phases of the ceramics are anorthite (JCPDS number 41-1486) and gehlenite (JCPDS number 01-0982) as shown in FIG. 7. The microstructure of the ceramic is seen in SEM picture, as shown in FIG. 8, the crystal grain is in narrow strip shape, sintering degree is not enough, and sintering neck is not dense. The porous anorthite/gehlenite complex-phase ceramic has the density of 1.71 g per cubic centimeter and the open porosity of 31.02 percent according to the test by the boiling method mentioned in the national standard GB/T3810.1-2006 ceramic tile test method. The flexural strength of the ceramic measured by the three-point bending method was 16.83 MPa. The volume of the blank prepared by the step (2) is V 0 When the volume of the ceramic obtained in step (3) is V, the volume shrinkage ratio ((V) 0 -V)×100%/V 0 ) Comprises the following steps: 30.43 percent.
Comparative example 2
The preparation method of the porous anorthite/gehlenite complex phase ceramic in the comparative example 2 is different from the preparation method in the example 1 in that only the mass part of the silicon carbide is changed into 0, namely, the silicon carbide is not added, and the preparation method specifically comprises the following steps:
(1) the materials are prepared according to the following mass portion ratio: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 9.96 parts of fused mullite powder and 3.32 parts of talc, adding water to ensure that the mass part ratio of the ingredients to the water is 100:80, drying the slurry for 2 hours at 110 ℃ after ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, manually manufacturing material particles, and taking the material particles below 100 meshes;
(2) placing the material particles prepared in the step (1) into a mold, forming under 200MPa, and drying at 110 ℃ for 2 hours to prepare a blank body;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃ at the speed of 6 ℃ per minute, preserving the heat for 2 hours, and cooling to room temperature to obtain the porous anorthite/gehlenite complex-phase ceramic.
Wherein:
the raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid in the step (1) mainly comprises 3.98% of CaO and Al 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO in sulfate form 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62 percent. The phases of the ceramics are anorthite (JCPDS number 41-1486) and gehlenite (JCPDS number 01-0982) as shown in FIG. 9. The microstructure of the ceramic is shown in SEM picture, as shown in figure 10, the crystal grain is well developed, the sintering neck is not compact, and a few holes are contained. According to the test of the boiling method mentioned in the national standard GB/T3810.1-2006 ceramic tile test method, the density of the porous anorthite/gehlenite complex phase ceramic is 1.34 g per cubic centimeter, and the open porosity is 51.49%. The flexural strength of the ceramic measured by the three-point bending method was 14.27 MPa. The volume of the blank prepared by the step (2) is V 0 When the volume of the ceramic obtained in step (3) is V, the volume shrinkage ratio is ((V) 0 -V)×100%/V 0 ) Comprises the following steps: 7.75 percent.
It can be seen from the comparative examples 1-2 that, when the porous anorthite/gehlenite complex-phase ceramic is prepared, when the other raw materials are unchanged, only the electric-melting mullite powder is not added in the comparative example 1, and the silicon carbide is not added in the comparative example 2, the volume shrinkage rate of the prepared porous anorthite/gehlenite complex-phase ceramic is greatly increased or the breaking strength is greatly reduced, and the volume shrinkage and the mechanical properties of the porous anorthite/gehlenite complex-phase ceramic cannot be balanced at the same time.

Claims (9)

1. A preparation method of porous anorthite/gehlenite multiphase ceramic with low firing shrinkage rate is characterized in that: the method comprises the following steps:
(1) weighing ingredients according to a certain mass part ratio, wherein the ingredients comprise feldspar, quartz, waste glass powder, waste brick powder, kaolin, sawdust, sodium tripolyphosphate, polyacrylic acid, calcium carbonate, alumina, fused mullite powder, silicon carbide and talc, adding water into the ingredients for ball milling, drying the obtained slurry, finally manufacturing material particles, sieving the material particles with a 100-mesh sieve, and taking the material particles which are sieved with the 100-mesh sieve;
(2) putting the material particles prepared in the step (1) into a die for compression molding, and drying to prepare a blank;
(3) and (3) heating the blank prepared in the step (2) to 1170 ℃, sintering, and cooling to room temperature to prepare the porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage.
2. The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the ceramic comprises the following steps: the ingredients in the step (1) comprise the following raw materials in parts by weight: 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of saw dust, 0.20 part of sodium tripolyphosphate, 0.32 part of polyacrylic acid, 23.90 parts of calcium carbonate, 18.92 parts of alumina, 9.96-18.11 parts of fused mullite powder, 0.33-0.66 part of silicon carbide and 3.32 parts of talc.
3. The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate as claimed in claim 2, wherein the ceramic comprises the following steps: in the step (1), a raw material mixture consisting of 11.59 parts of feldspar, 10.27 parts of quartz, 7.62 parts of waste glass powder, 6.95 parts of waste brick powder, 4.97 parts of kaolin, 1.32 parts of sawdust, 0.20 part of sodium tripolyphosphate and 0.32 part of polyacrylic acid comprises 3.98% of CaO and 0.32% of Al in main chemical composition 2 O 3 12.1%、SiO 2 59.9% CO in carbonate 2 12.1%、B 2 O 3 4.24%、Na 2 O 1.81%、Fe 2 O 3 1.39% SO measured as sulphate 3 1.26%、K 2 O1.17%, MgO 0.74%, NO measured as nitrate 2 0.62%。
4. The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the ceramic comprises the following steps: the mass part ratio of the ingredients to the water in the step (1) is 100: 80.
5. The preparation method of the porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the preparation method comprises the following steps: and (2) adding water into the ingredients in the step (1) and carrying out ball milling for 1h at the speed of 400 r/min.
6. The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the ceramic comprises the following steps: and (2) drying the obtained slurry in the step (1) at 110 ℃ for 2 h.
7. The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the ceramic comprises the following steps: in the step (2), the forming pressure is 200MPa, the drying temperature is 110 ℃, and the drying time is 2 h.
8. The preparation method of the porous anorthite/gehlenite complex-phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the temperature is raised to 1170 ℃ at the speed of 6 ℃/min for sintering, and the temperature is kept for 2 h.
9. The preparation method of the porous anorthite/gehlenite complex phase ceramic with low firing shrinkage rate as claimed in claim 1, wherein the ceramic comprises the following steps: the cooling to room temperature in the step (3) is furnace cooling.
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US4808460A (en) * 1987-06-02 1989-02-28 Corning Glass Works Laminated structures containing an inorganic corrugated or honeycomb member
CN107628819A (en) * 2016-07-18 2018-01-26 北方民族大学 A kind of method for the porous material that the phase containing melilite is prepared using magnesium slag, flyash, carbide slag
JP2018165224A (en) * 2017-03-28 2018-10-25 佐賀県 Porous ceramic
CN111978100A (en) * 2020-07-13 2020-11-24 南通大学 Preparation and performance improvement method of anorthite/gehlenite complex phase ceramic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4808460A (en) * 1987-06-02 1989-02-28 Corning Glass Works Laminated structures containing an inorganic corrugated or honeycomb member
CN107628819A (en) * 2016-07-18 2018-01-26 北方民族大学 A kind of method for the porous material that the phase containing melilite is prepared using magnesium slag, flyash, carbide slag
JP2018165224A (en) * 2017-03-28 2018-10-25 佐賀県 Porous ceramic
CN111978100A (en) * 2020-07-13 2020-11-24 南通大学 Preparation and performance improvement method of anorthite/gehlenite complex phase ceramic

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